Dinitroglycerin explosive and process of making.



vantages,- a' number of-pro'c'esseshave been manns'frnrns en ran s enricarer insersczinor erases-r.

anti-assessment" nfinosrv'n rnoenss or M AmNG.

specification of Letters Patent.

Patented Jan. 26, 190 9.

Griginal e nmaoseiea April is, 1904, Serial in. 203,762. Pivid ed. andthis application filed October 25, less.

. p Serial No. aaassr;

To e22 sama'may concern;-

Be it known that I, ANTON MrKoLAJozAK, a subject of the King of Prussia,residing at Kastrop, in the Province of est'phalia and 5 German Empire,have invented a new and useful Dinitroglycerin- Explosive and Proc' essof Making It, of which the following is a specification.

This invention relates to the manufacture a of explosives containing"dinitroglycerin and is a division of my application Ser. No.

203,762, upon which Patent No. 7 98,436 Was issued to me on Augf29,1905.

According to the practice prevailing in the 5 manufacture of dynamite,carbonite and other nitroglycerin explosives prior to my invention thenecessary nitroglycerin is prepared in-the form of trinitroglycerin ofas pure 2. character as possible, by nitroglycerin the glycerintri-nitrate (J E (O,NO )3 being understood.

This nitroglycerin, also known as blasting o1l ,.acccrding to theordinary method of preparation may unintentionally have been mixed witha small quantity of less nitrated compound glycerin ethersor'dinitroglycerin, but the presence of the lower nitrates in the:trinitroglycerin has been a matter of conjecture rather than groof andthey have been su posed to be a etri-ment to the explosive. am the firstto have isolateddin troglycerin and studied its. propcr tics, and havediscovered means of producing. and isolating it; .and I have also dis- 5eovereditsjmanydesirable and highly mi-- liable characteristics inemploying-s it in the manufacture of explosives. I

erin consist in the h sens 'tyof thesub o stance tomechariica shocks andheat, in the readmem with whichi-tfreezes, and the like.- Theyiead to dfliculties both in its manu- The disadvantages adhenibpfi1 to nitroglyce.

fracture and in its application and are-the;

cause ofmany accidents;

For the purpose of removing these disadinvented. I may mention herethatof mixmgmtro-benzol, amyl-nitrate, etc. Most of ese recesses, however,have'proved a to-- 5o tal fa ure, while others have not been-em 'ployed-witlr-real successinpractice;

the employment of: dini-troglycerin :5 herein-seated a pioeess ofm n f'l quantities, does not cause explosion, as

while nitroglycerin lixiviated from comfor SllOOtlJlfi and blastingpurposes.

expldsives which ,offers great advantages over the processes referred tofor the following reasdnss- 1.. Dinitroglycerin is a considerably morestable com oundthan the extremely unstable blasting oil,trinitroglycerm,

It is, therefore",'rriuch less sensible to shock and heat than thelatter. Pure -dinitr'oglycerin does not e lode on ignition at all. By.adding a gradua y increasin percentage of 'dinitroglycerin to trinitrogycerin, the dangerous characteristics of the latter can be more and morediminished.

2. Dinitroglycerin can' be prepared altogether without danger, sinceanydecomposition accidentally occurring in -the course of manufacture,even in the caseof very large numerous experiments, where dccom osivtionhas been purposely brought about, ave

proved. J

3. Dinitroglycerin for all practical pburoses may be considered asuncongeala le. ts addition .to trinitroglycerin lowers thefreezing-point of the latter to such. an extent that a mixture of, forinstance, 60% dinitroand 4 0% trinitro lycerin was" found to remainperfectly Enid during severe frost,-

mercial dynamites, as well as the latter themselves, froze completelyunder the same experimental conditions.

4. By the selection of suitable quantities 2 of dinitroglycerin andordinaryblasting oil,

an oil can be produced superior to ordinary blasting oil in explosivepower. For nitroglycerin contains more oxygen than is necessary for acomplete combustion of its carbon to carbonic acid, and of its hydrogento water, whiledinitroglycerin contains too little. Thus, by mixingthese two compound ethers a product equalizing these two conditionscan'be obtamed, which may be regarded as an ideal blasting oil andwhereby the greatest possible explosive force is ob-: tained. 5.- Whathas been said inaragraphs 1, 3 and- 4 in res ect to dinitrog lycen'nandits mixtures with blasting-oil naturally applies also'to allexplosives-prepared from the same In the explosive powders for shoot"case of suc or military purposes there is the additiona 1-10 advantagethat on account of the lower tem- 'i. 45. dinitrogl cerin perature ofthe enerated gases, which are 30. 0% -trinitrog ycerin also much moresowly generated, the barrel 2. 0% chalk of the gun-is attacked to a muchless degree 23. 0% infusorial earth (kleselguhr) 5 than in the case ofthe well-known nitro- .7- glycerin powders. 100. 0%

6. Dimtroglycerin is readily soluble in k 41 dinitrou] crin everyproportion in nitroglycerin, and any trinitm" Carin suitagblemixtufiedef dil and trinitroglycerin chalk g y p 75' 10 can e re areirect i 7. Diiiit oglycerin is j ust as good a solvent 0% mfusonal earth(kie-selguhr) and gelatim'zing medium for various sub- 10607 stancessuch as nitro-cellulose, xyloidin, etc. 0 as is trinitroglycerin. v Z.14- 0% dinitr gl fi i 15 I The follouing examples of explosives may 78.0% trinitrog ycerin 80 be here given '8. 0% solublapyroxylin a 61. 0 I 0f stateless... I Potasslum filtrate Y m. 12. 5% dinitroglycerin I 85Wood-meal 62. 5% tainlilgroglycerin' 1 v 1. 0% c a b 100. 0;, d 1 I 24.0% infusorial earth (kieselguhri 38.4 o initro cerin '25. 6%blasting-iii] (trinitroglycerin) 0 90 1. 7% soluble pyr yl As an exampleof m method of manufac 27. 0% sodium nitrate I turin dinitroglycerin maycite the follow:

7.3% Wood-meal ing: 0- 10 parts by weight of glycerin, 7 1 r1.2(f21sp8c.gr., 33 parigdbyiweilghtbo filitric v ac] spec. gr. area e-e1t e r y oW- 95 c. 17.0% dinitroglycerin ing the nitric acid to slowlyflow into the 58. 0% blasting-oil glycerin, or the glycerin into thenitric ecid. 23. 0% infusorial earth (kieselguhr) During this operationthe two liquids are 2. 0% chalk. v l thoroughly mixed by stirring andthe tem- 3 35 erature of the mixture is kept preferably 100 100.0%elowhlfif; to 18 C. Thle mixture-climtatllrc 'e ymono-nitrog ycerin is-t en v lowed to stand for some time (it maybe J 1 0% di Phenymm-in vseveralhours) by preference at .a temper- 40 ature not above 20C.,-.unt1l the mon0--105 07 nitroglycerin is converted into dinitr0 0 egl cerln. The entire mass is then diluted. e. 20.0% dmltroglycerm Wlthabout 10 parts by weight of cold water.

9 py y i and the nitric acid neutralized by a suitable 4 I v agent'untilthe lye, .for example in case of 0- r using carbonate of lime for'neutralization f. 40'. 0% dinitroglycerin has a specific gravity of1.58. The 'dinitroe I 10. 0% blasting-oil glycerin rises therein, andcan be read1Iy- 49.0% soluble pyroxylin separated, purified and dried.50 1 0% di h 1 mi v Any 'dimtroglycerin which ma remam e in the .lye'canbe readily'removed' y means 1.00. 0% pf a selvent, suteh gs eltlher,andlfogta ineid j- 7 rom tie atter isti ation. t eslre I i p ythemixture of 'oil andlye deprived ofacid, 55 1"; i t can be treatedin thesame manner without mg g ig I rior separatipln, no technicaldifficulties p elng presente Dimtroglycerin .s obtained as a colorless0% oil when the l cerin andthe nitric acid are 60 h. 7. 5% ,dinitroglc'erin colorless, that ig to say free from impurities;

42. 5% trinitrog ycerin It is, soluble in water tea large extent and.49. 0%; soluble p roxylin .bg'reason' of this property can very wellbe 1. 0%. d1-pheny amin o tain'ed quite pure, for instance, by free-- 65-tional evaporation of thewat'en, The-well I known solvents fornitroglycerin also readily 13 0 absorb dinitroglycerin. The percentageof nitrogen according to calculation is 15.38; an actual analysis(nitrometer and organic analysis) showed the average to be 15.38 percent.

If mixtures of dinitroglycerin with trinitroglycerin are employed formanufacturing explosives or gun powder, the dinitroglycerin can firstbe-prepared separately and then mixed If, however, a suitable mixture ofnitric acid and sulfuric acid of certain nitrifying efiiciency ornitration value is made, said mixture may be used for preparing andobtaining direct a mixture of both the trinitroglycerin and thedinitroglycerin, i. e. a mixture containing the desired percentage ofdinitroglycerin.

To manufacture ex losives for commercial use from dinitrog ycerin, or amixture of diand tri-nitroglycerin, which are comparatively mobileliquids, it is necessary, to either absorb the liquid in a suitablematerial, or thicken it by a gelatinatin medium. The bodies obtained byeither of these processes are mixed with a solid inorganic oxidizingsalt, such as the nitrates of sodium, potassium, ammonium, barium, orchlorates, perchlorates, etc., preferably in finely powdered form, in asuitable kneading apparatus. The dough-like mass is fed into a cartridgemachine.

The process of manufacturing such a mix- I ture of glycerin nitrates ismore fully described and claimed in my 00- ending application, Serial N0. 239,732, file January 5th, 1905. i

I/Vhat I claim as my invention and desire to secure by Letters Patentis 1. In the process of manufacturing explosives the step which consistsin dissolving gelatinating media in dinitroglycerin to increase 1tsvlscosity.

2. The process of manufacturing exploing media in a mixture of diandtri-nitrosiveswhich consists in" dissolving gelatinating media indinitroglycerin and incor orating solid inorganic oxidizing salt,,-witsaid mixture.

3. The rocess of manufacturing explosives whic consists in dissolvinggelatinating media in dinitroglycerin, incorporatin solid inorganicoxidizing salt therewith an adding to said mixture carbonaceousmaterial.

4. In the process of manufacturing explosives the step which consists indissolving gelatinating media in a mixture of diand tri-nitroglycerin toincrease its viscosity.

5. The rocess of manufacturing explosives, whic consists in dissolvinggelatinat-.

glycerin and incorporating solid inorganic oxidizing salt therewith. f

6. The rocess of manufacturing explosives, whic consists in dissolvinggelatinating media in a mixture of diand tri-nitro- 'glycerin,incorporating solid inorganic oxiconstituents.

8. As a new article of manufacture an explosive, consisting of a mixtureof diand trinitroglycerin and a solid inorganic oxidizing salt, andcarbonaceous material In testimonywhereof I have signed my name to thisspecificationin the presence of two subscribing Witnesses.

ANTON MIKOLAJCZAK.

Witnesses PAUL Mr'iLLER, Lunwio KLEIN.

